生体試料中の総水銀分析を目的とした試料燃焼方法の改良
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Combustion methods for the determination of mercury are known to be better suited to biological materials. But main disadvantage of these methods is that the amount of sample is limited to quite a small extent to attain the complete combustion. The main purpose of this study was to increase the upper limit of the amount of sample needed for the combustion method for the determination of mercury. The combustion apparatus was modified as shown in Fig. 1, in which samples were first pyrolyzed in the stream of nitrogen {(0.2〜0.3)1/min} during the rise of temperature up to about 800℃. The pyrolysis gas thus formed was introduced to the combustion zone where organic components were completely oxidized under the stream of oxyeen {(1.8〜2.0)1/min}. Up to about 0.5 gram of dry sample or 1.2grams of raw fish tissues were found to be easily subjected to the complete combustion within 5 minutes. Mercury was quantitatively released from the sample during the pyrolysis, and after the removal of cocxistent interference gases by flowing the combustion gas through a column packed with sodium carbonate granules, mercury was introduced into silver amalgamator and trapped there. On heating the amalgam, mercury vapor was released again and was determined by the flameless atomic absorption spectrometry. Good agreements were found between the results of the present method and reference values. Abnormal analytical values which are often obsereved in the oxidative combustion techniques which are accompanied with flare of samples can be eliminated by this method.
- 社団法人日本分析化学会の論文
- 1978-01-05
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